JPS5994828A - Etching solution for silicon crystal evaluation - Google Patents
Etching solution for silicon crystal evaluationInfo
- Publication number
- JPS5994828A JPS5994828A JP20481082A JP20481082A JPS5994828A JP S5994828 A JPS5994828 A JP S5994828A JP 20481082 A JP20481082 A JP 20481082A JP 20481082 A JP20481082 A JP 20481082A JP S5994828 A JPS5994828 A JP S5994828A
- Authority
- JP
- Japan
- Prior art keywords
- etching
- volume
- defects
- solution
- silicon
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 238000005530 etching Methods 0.000 title claims abstract description 48
- 239000013078 crystal Substances 0.000 title claims abstract description 19
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 title claims abstract description 16
- 229910052710 silicon Inorganic materials 0.000 title claims abstract description 15
- 239000010703 silicon Substances 0.000 title claims abstract description 15
- 238000011156 evaluation Methods 0.000 title claims abstract description 11
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims abstract description 31
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims abstract description 29
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract description 16
- 229910017604 nitric acid Inorganic materials 0.000 claims abstract description 16
- 239000011259 mixed solution Substances 0.000 claims abstract description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 4
- 239000007788 liquid Substances 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 2
- 239000000243 solution Substances 0.000 abstract description 24
- 230000007547 defect Effects 0.000 abstract description 17
- 239000012535 impurity Substances 0.000 abstract description 16
- 239000000758 substrate Substances 0.000 abstract description 5
- 238000000034 method Methods 0.000 abstract description 4
- QPJSUIGXIBEQAC-UHFFFAOYSA-N n-(2,4-dichloro-5-propan-2-yloxyphenyl)acetamide Chemical compound CC(C)OC1=CC(NC(C)=O)=C(Cl)C=C1Cl QPJSUIGXIBEQAC-UHFFFAOYSA-N 0.000 abstract description 4
- IOVCWXUNBOPUCH-UHFFFAOYSA-N Nitrous acid Chemical compound ON=O IOVCWXUNBOPUCH-UHFFFAOYSA-N 0.000 abstract 1
- 229960000583 acetic acid Drugs 0.000 description 7
- 239000000203 mixture Substances 0.000 description 6
- 239000004065 semiconductor Substances 0.000 description 4
- 230000000694 effects Effects 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 2
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- TUCNEACPLKLKNU-UHFFFAOYSA-N acetyl Chemical compound C[C]=O TUCNEACPLKLKNU-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910052796 boron Inorganic materials 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 239000012362 glacial acetic acid Substances 0.000 description 1
- 229910000040 hydrogen fluoride Inorganic materials 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 150000003376 silicon Chemical class 0.000 description 1
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
- H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic Table or AIIIBV compounds with or without impurities, e.g. doping materials
- H01L21/30—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26
- H01L21/302—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26 to change their surface-physical characteristics or shape, e.g. etching, polishing, cutting
- H01L21/306—Chemical or electrical treatment, e.g. electrolytic etching
Landscapes
- Engineering & Computer Science (AREA)
- Physics & Mathematics (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Manufacturing & Machinery (AREA)
- Computer Hardware Design (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Power Engineering (AREA)
- Weting (AREA)
Abstract
Description
【発明の詳細な説明】
（１）発明の技術分野
本発明はシリコン（Ｓｌ）結晶評価に用いる選択エツチ
ング液の改良に関する。DETAILED DESCRIPTION OF THE INVENTION (1) Technical Field of the Invention The present invention relates to improvement of a selective etching solution used for silicon (Sl) crystal evaluation.
（２）技術の背景
半導体プロセス評価技術の一つとして、半辱体ノエッチ
ングレートが結晶状態の良否に対応して変化する現象を
利用して、板状体の半導体に対しエツチングを施したの
ち、倍率が１．０００倍程度の光学顕微鏡、または、倍
率が数百倍程度の走査型電子顕微鏡（ＳＥＭ）等を使用
して表面の凹凸を観察して半導体の結晶状態を評価する
技術があり、結晶欠陥等を直接目視しつる方法として広
く利用されている。(2) Background of the technology As one of the semiconductor process evaluation technologies, a semiconductor plate is etched by taking advantage of the phenomenon that the etching rate of semicircular bodies changes depending on the quality of the crystalline state. There are techniques for evaluating the crystalline state of semiconductors by observing surface irregularities using an optical microscope with a magnification of about 1.000 times or a scanning electron microscope (SEM) with a magnification of several hundred times. , is widely used as a method for directly visualizing crystal defects, etc.
（３）従来技術と問題点
かかる結晶欠陥観察の目的をもってなすエツチングに使
用するエツチング液としては、従来、セ、ｙ ：ｌ （
５ｅｃｃｏ）エツチング液、ジルトル（Ｓｉｒｔｌ）エ
ツチング液、ダッシュ（Ｄａｓｈ）エツチング液等が利
用されていた。ところが、半導体装置の表面には導電型
及び／又は不純物濃度を異にする領域があるため、上記
のセック（Ｓｅ ｃｃｏ）エラ−Ｆ−７ダ液、ジルトル
（Ｓｉｒｔｌ）エツチング液を使用して結晶状態の評価
をなす場合、ｎ型不純物を含む領域とｎ型不純物を含む
領域とのエツチングレートが太き（異なり、その結果、
ｎ型不純物を含む領域の観察に適するエツチングがなさ
れた状態においては、ｎ型不純物を含む領域のエツチン
グが未完で観察が困難であり、一方、逆にｎ型不純物を
含む領域の観察に適するエツチングがなされた状態にお
いてはｎ型不純物を含む領域の観察が不可能となる。換
言すれば、ｎ型不純物を含む領域の観察を完了したのち
、更にエツチングを続行してｎ型不純物を含む領域の観
察を行なう必要があり、操作が煩雑で現実的ではない。(3) Prior art and problems The etching solution used for etching for the purpose of observing crystal defects has conventionally been
5ecco) etching solution, Sirtl etching solution, Dash etching solution, etc. were used. However, since there are regions on the surface of a semiconductor device with different conductivity types and/or impurity concentrations, the above-mentioned Secco Error-F-7 dazzling solution and Sirtl etching solution are used to improve the crystallization. When evaluating the condition, the etching rate of the region containing n-type impurities and the region containing n-type impurities are thicker (different, and as a result,
In a state where etching suitable for observation of a region containing n-type impurities has been performed, the etching of the region containing n-type impurities is incomplete and observation is difficult; In this state, it becomes impossible to observe a region containing n-type impurities. In other words, after completing the observation of the region containing the n-type impurity, it is necessary to continue etching to observe the region containing the n-type impurity, which is a complicated operation and is not practical.
また、ダッシュ（Ｄａｓｈ）エツチング液は、全体とし
てのエツチングレートが、上記２つのエツチング液より
２桁小さく、エツチングに長時間を要し、しかも、ｐ生
型領域にスティン膜が容易に形成されてその部分のエツ
チングが進行しないという欠点がある。In addition, the overall etching rate of the Dash etching solution is two orders of magnitude lower than that of the above two etching solutions, and it takes a long time for etching.Moreover, a stain film is easily formed in the p-type region. The disadvantage is that etching does not progress in that area.
（４）発明の目的
本発明の目的は、上記の３種のエツチング液の有する欠
点をすべて解消することにあり、欠陥に対するエツチン
グ選択性を有し、しかも、そのエツチングレートが導電
型及び／又は不純物濃度に依存しない、シリコン（Ｓｉ
）結晶評価用エツチング液を提供することにある。(4) Purpose of the Invention The purpose of the present invention is to eliminate all the drawbacks of the three types of etching solutions mentioned above, to have etching selectivity for defects, and to have an etching rate that is suitable for conductivity type and/or Silicon (Si) does not depend on impurity concentration.
) To provide an etching solution for crystal evaluation.
（５）発明の構成
本発明の構成は、０．０３〜０．１３ ［容］の弗酸（
ＨＦ）と、０，２６〜０．６１（容〕の硝酸（）ＩＮ（
Ｊ ３）と、酢酸（ＣＨ３ｅｏｏｉ−ｉ）とを含有し、
全体として１容となる混合液１容と０３〜０．７容の水
（Ｈ２Ｏ）とを混合してなることを特徴とする、シリコ
ン（Ｓｌ）結晶評価用エツチング液にある。(5) Structure of the invention The structure of the present invention consists of 0.03 to 0.13 [volume] of hydrofluoric acid (
HF) and 0.26-0.61 (volume) nitric acid ()IN(
J3) and acetic acid (CH3eooi-i),
An etching solution for silicon (Sl) crystal evaluation is characterized in that it is made by mixing 1 volume of a mixed solution and 0.3 to 0.7 volumes of water (H2O) to make a total of 1 volume.
本発明の発明者は、エツチングレートの不純物濃度依存
性や欠陥に対する選択性は、上記エツチング液の構成要
素のうち主として硝酸（ＨＮ（Ｊ、）と一部弗酸（ＨＦ
）の容量比によって決定されることを実験的に見出した
。すなわち、上記の構成において、硝酸（ＨＮ（Ｊ３）
の容量比を０．２６以下とすると、他の２つの構成要素
の容量比如何にかかわらず、エツチングレートが不純物
濃度に大きく依存し、一方、硝酸（ＨＮＯ３）の容量比
が０６１以上で、かつ、弗酸（ＨＦ ）の容量比０．１
３以上とすると、欠陥に対する選択性が失なわれる。し
たがって、以上の事実から１本発明の発明者は夫々の容
量比を上記構成に示した範囲から選択することとして本
発明を完成した。The inventor of the present invention has determined that the impurity concentration dependence of the etching rate and the selectivity for defects are determined by using mainly nitric acid (HN (J)) and a portion of hydrofluoric acid (HF) among the components of the etching solution.
) was determined experimentally by the capacity ratio of That is, in the above configuration, nitric acid (HN(J3)
When the capacity ratio of nitric acid (HNO3) is 0.26 or less, the etching rate largely depends on the impurity concentration, regardless of the capacity ratio of the other two components; , hydrofluoric acid (HF) capacity ratio 0.1
When the number is 3 or more, selectivity for defects is lost. Therefore, based on the above facts, the inventor of the present invention completed the present invention by selecting each capacitance ratio from the range shown in the above configuration.
また、本発明に係るエツチング液の構成要素である弗酸
（１（Ｆ）、硝酸（）ＩＮＯ，）、氷酢酸（ＣＨ３ＣＯ
（ＪＨ）は、いずれも市販品を使用することが現実的で
あるが、夫々の含有率を考慮し、上記構成に示した容量
比となるよう調製して用いる必要があることは言うまで
もない。In addition, hydrofluoric acid (1(F), nitric acid ()INO,), glacial acetic acid (CH3CO,
Although it is practical to use commercially available products for each of (JH), it goes without saying that it is necessary to consider the content of each and adjust the volume ratio as shown in the above structure.
以上、本発明によれば、欠陥に対するエツチング選択性
は良好であり、かつ、セック（５ｅｃｃｏ）エツチング
液、ジルトル（５ｉｒｔｌ）エラ−ｆ−７りＭの欠点で
あるエツチングレートの不純物濃度依存性は改善され、
さらに、ダッシュ（Ｄａｓｈ）エツチング液の欠点であ
るエツチングレートが遅い点は、値にして２桁向上し、
また、上記構成に示された容量比の範囲ではスティン膜
の形成を伴なわないエツチング液を実現でき、結果とし
て結晶評価を望ましい状態で実行することができる。As described above, according to the present invention, the etching selectivity for defects is good, and the impurity concentration dependence of the etching rate, which is a drawback of the 5ecco etching solution and the 5irtl etchant, is eliminated. improved,
Furthermore, the slow etching rate, which is a drawback of Dash etching liquid, has been improved by two orders of magnitude.
Further, within the range of the capacitance ratio shown in the above configuration, an etching solution that does not involve the formation of a stain film can be realized, and as a result, crystal evaluation can be performed in a desirable state.
（６）発明の実施例 次に本発明の実施例について説明する。(6) Examples of the invention Next, examples of the present invention will be described.
シリコン基板にトランジスタを作成し、その素子特性を
測定した後、シリコン基板から電極及び酸化膜を除去し
、シリコン結晶を露出させる。この時、ベース領域には
硼素が５×１０１８０Ｉｎ−３、またエミッタ及びコレ
クタ領域には燐が１Ｘ１０ｃ＋ｎ拡散されている。この
シリコン基板を弗酸、硝酸、酢酸の容量比１：５：５の
組成液で３０秒間エツチングしたところ、すべての領域
において欠陥が観察できるようになり、素子特性と結晶
欠陥との関連を観測出来た。After forming a transistor on a silicon substrate and measuring its device characteristics, the electrodes and oxide film are removed from the silicon substrate to expose the silicon crystal. At this time, 5 x 10180 In-3 of boron is diffused into the base region, and 1 x 10 c+n of phosphorus is diffused into the emitter and collector regions. When this silicon substrate was etched for 30 seconds with a solution containing hydrofluoric acid, nitric acid, and acetic acid in a volume ratio of 1:5:5, defects could be observed in all regions, and the relationship between element characteristics and crystal defects was observed. done.
また、弗酸、硝酸、酢酸の容量比Ｊ：１０：５の組成液
でも同様の効果が得られた。更に弗酸、硝酸、酢酸の容
量比１：１０：１０の組成液では、１分間のエツチング
で同様の効果が得られた。Further, a similar effect was obtained with a liquid composition having a volume ratio of hydrofluoric acid, nitric acid, and acetic acid of J:10:5. Furthermore, with a composition solution containing hydrofluoric acid, nitric acid, and acetic acid in a volume ratio of 1:10:10, a similar effect was obtained after etching for 1 minute.
表は本実施例の組成液を用いて１分間エツチングした時
のエミッタ、ベース、コレクタ各領域のエツチング量を
示す。The table shows the amount of etching in the emitter, base, and collector regions when etching was performed for 1 minute using the composition solution of this example.
なお、本発明の範囲外の組成液を用いてエツチングを行
った場合１．硝酸の容量比０．３５以下ではエツチング
速度が不純物濃度に大きく依存し、また、硝酸の容量比
０．７以上及び弗酸の容量比０．１５以上では欠陥に対
する選択性が失なわれるため好ましくない。Note that if etching is performed using a composition solution outside the scope of the present invention, 1. If the volume ratio of nitric acid is 0.35 or less, the etching rate largely depends on the impurity concentration, and if the volume ratio of nitric acid is 0.7 or more and the volume ratio of hydrofluoric acid is 0.15 or more, selectivity to defects is lost, so it is preferable. do not have.
なお、組成液を弗酸、硝酸、酢酸の濃度の異なる液から
調整した場合でも、それぞれ、弗化水素分、硝酸分、酢
酸分が本発明の範囲内であれば同様の効果がある。Note that even when the composition liquid is prepared from liquids having different concentrations of hydrofluoric acid, nitric acid, and acetic acid, the same effect can be obtained as long as the hydrogen fluoride content, nitric acid content, and acetic acid content are within the range of the present invention.
本発明の組成液は、エツチング速度が不純物濃度にあま
り依存せず、かつ、結晶欠陥に対する選択性があるので
、不純物拡散等を行ない、トランジスタ等の素子を作成
した、シリコン基板に用いた場合、どの領域においても
結晶欠陥が観察できるようになるため、素子の電気的特
性と、結晶欠陥との対応を知ることができる。The composition solution of the present invention has an etching rate that does not depend much on the impurity concentration and is selective to crystal defects, so when it is used on a silicon substrate on which an element such as a transistor is made by performing impurity diffusion, etc. Since crystal defects can be observed in any region, it is possible to know the correspondence between the electrical characteristics of the device and the crystal defects.
また、エツチング時間が３０秒〜１分間と短かく、また
、エツチング量が１〜２ 〔μ＋ｎ）で欠陥を観察でき
るため、素子作成部分の評価が出来るという効果がある
。さらに、薄いエピタキシャル成長層の評価にも有効で
ある。Furthermore, since the etching time is short, 30 seconds to 1 minute, and defects can be observed with an etching amount of 1 to 2 [μ+n], it is possible to evaluate the device fabrication area. Furthermore, it is also effective for evaluating thin epitaxial growth layers.
ＩＮＦ：ＨＮＯａ： エミッタ領域 ベース領
域 コレクタ領域ＣＨａＣＯＯＨ
１：５：５ １゜７５〔μ＋ｎ〕１．５６［μ’ｎ
） １．５６ （μｒｎ）１ ： １０ ：
５ ２．００ １．７６ １．７１
１ ： １０ ： １０ ０．９３ ０．
２４ ０．７９（力発明の詳細
な説明せるとおり、本発明によれば、欠陥に対するエツ
チング選択性を有し、しかも、そのエツチングレートが
導電型及び／又は不純物濃度に依存しない、シリコン（
Ｓり結晶評価用エツチング液を提供することができる。INF:HNOa: Emitter region Base region Collector region CHaCOOH 1:5:5 1°75 [μ+n] 1.56 [μ'n
) 1.56 (μrn) 1: 10:
5 2.00 1.76 1.71
1: 10: 10 0.93 0.
24 0.79 (According to the present invention, as described in detail, silicon (
An etching solution for evaluating S crystals can be provided.
Claims (1)
．６１容の硝酸と、酢酸とを含有し、全体として１容と
なる混合液１容と０．３容乃至０．７容の水とを混合し
てなることを特徴とする、シリコン結晶評価用エツチン
グ液。0.03 volume to 0.13 volume of hydrofluoric acid and 0.26 volume to 0.
．． For silicon crystal evaluation, characterized by being made by mixing 1 volume of a mixed solution containing 61 volumes of nitric acid and acetic acid, making a total of 1 volume, and 0.3 to 0.7 volumes of water. Etching liquid.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP20481082A JPS5994828A (en) | 1982-11-22 | 1982-11-22 | Etching solution for silicon crystal evaluation |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP20481082A JPS5994828A (en) | 1982-11-22 | 1982-11-22 | Etching solution for silicon crystal evaluation |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPS5994828A true JPS5994828A (en) | 1984-05-31 |
Family
ID=16496739
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP20481082A Pending JPS5994828A (en) | 1982-11-22 | 1982-11-22 | Etching solution for silicon crystal evaluation |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS5994828A (en) |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH02268468A (en) * | 1989-04-10 | 1990-11-02 | Casio Comput Co Ltd | Thin film transistor and manufacture thereof |
| DE4305297A1 (en) * | 1993-02-20 | 1994-08-25 | Telefunken Microelectron | Texturing pickle for semiconductors, and use thereof |
| US5943549A (en) * | 1996-12-27 | 1999-08-24 | Komatsu Electronics Metals Co., Ltd. | Method of evaluating silicon wafers |
| WO2006080264A1 (en) * | 2005-01-27 | 2006-08-03 | Shin-Etsu Handotai Co., Ltd. | Method of selective etching and silicon single crystal substrate |
| KR100646730B1 (en) | 2004-12-29 | 2006-11-23 | 주식회사 실트론 | Etching solution for evaluating crystral faults in silicone wafer and evaluation method using the same |
| EP1926132A1 (en) * | 2006-11-23 | 2008-05-28 | S.O.I.Tec Silicon on Insulator Technologies | Chromium-free etching solution for Si-substrates and SiGe-substrates, method for revealing defects using the etching solution and process for treating Si-substrates and SiGe-substrates using the etching solution |
| CN111019659A (en) * | 2019-12-06 | 2020-04-17 | 湖北兴福电子材料有限公司 | Selective silicon etching liquid |
-
1982
- 1982-11-22 JP JP20481082A patent/JPS5994828A/en active Pending
Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH02268468A (en) * | 1989-04-10 | 1990-11-02 | Casio Comput Co Ltd | Thin film transistor and manufacture thereof |
| DE4305297A1 (en) * | 1993-02-20 | 1994-08-25 | Telefunken Microelectron | Texturing pickle for semiconductors, and use thereof |
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